HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → [1,1'-Biphenyl]-4-yl-(5,11-dihydro-10H-dibenzo[b,e][1,4]diazepin-10-yl)methanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | 10,11-Dihydro-5h-dibenzo[b,e][1,4]diazepine | HCID 36046 | — |
| Edukt | 4-Phenylbenzoyl chloride | HCID 84151 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | [1,1'-Biphenyl]-4-yl-(5,11-dihydro-10H-dibenzo[b,e][1,4]diazepin-10-yl)methanone | HCID 9821040 | 38,3% |
Reaktionsschritte
4-Biphenyl-carbonyl chloride (1.19 g) dissolved in N,N-dimethylformamide (10 mL) was added dropwise to an ice cooled solution of 5,11-dihydro-10H-dibenzo[b,e][1,4]diazepine (0.98 g) in N,N-dimethylformamide (10 mL). After stirring at room temperature overnight, the reaction mixture was poured into water and dichloromethane. The organic layer was sequentially washed with water and saturated sodium bicarbonate, and dried over anhydrous sodium sulfate. The solution was filtered through a short column of Magnesol® and eluted with additional dichloromethane. The combined eluate was refluxed with gradual addition of hexane until incipient crystallization occurred. Cooling and filtration provided the title compound (0.72 g), m.p. 180-182° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06903091B2 |
| Quelldatensatz | uspto-grants-2005_06 |
| ORD ID | ord-e38868efe6cf4a08b576ea1e4028954e |
| Quellennotiz | uspto-grants-2005_06 |